化工社化工社 化学情報印刷レポート · 研究参考用
Acetone → 2-(6-Bromo-5-methoxypyridin-2-yl)propan-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Bromo-6-iodo-3-methoxypyridine | HCID 11099040 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(6-Bromo-5-methoxypyridin-2-yl)propan-2-ol | HCID 57556073 | — |
反応手順
2-Bromo-6-iodo-3-methoxy-pyridine (500 mg) is dissolved in dry toluene (5 ml) and thereto is added dropwise 1.6M n-butyllithium in hexane (1 ml) at −78° C. under nitrogen atmosphere, and the mixture is stirred for 1 hour and thereto is added acetone (0.23 ml), and the mixture is stirred overnight. To the reaction solution are added water and ethyl acetate, and the mixture is separated, and the organic layer is washed with a saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=4:1→6:2) to give 2-(6-bromo-5-methoxy-pyridin-2-yl)-propan-2-ol (197 mg). MS (m/z): 246/248 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08076364B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-1f6e356549924bf58356ad7926f353d7 |
| 出典メモ | uspto-grants-2011_12 |